高效液相色谱法检测牛奶中的氟哌啶醇残留

Determination of haloperidol in milk by high performance liquid chromatography

目的建立高效液相色谱法检测牛奶中氟哌啶醇残留量的分析方法。方法样品采用酸化乙腈(0.2%甲酸,V:V)提取,C18固相萃取小柱净化,氮吹浓缩后,经0.45μm滤膜过滤,使用安捷伦ZORBAX SB-C_(18)色谱柱进行分离,乙腈-0.2%甲酸水溶液(1:1,V:V)作为流动相以0.3 mL/min流速等度洗脱,外标法定量。结果经选择,紫外检测波长为254 nm,此条件下,氟哌啶醇质量浓度(X,μg/mL)与其峰面积(Y)在0.2~5.0μg/mL范围内,线性关系良好,相关系数为0.999,在3.0、7.0、10.0μg/mL 3水平的加标回收率为81.73%~95.57%,相对标准偏差为1.97%,检出限为7.58μg/L,定量限为25.27μg/L。结论此方法具有成本低、操作简单、可操作性强、回收率高、灵敏度高、精确度高等优点,适用于牛奶中氟哌啶醇的检测。

Objective To establish a method for the determination of haloperidol residues in milk by high performance liquid chromatography.Methods The samples was extracted with acidified acetonitrile(0.2% formic acid,V:V),purified by C18 solid phase extraction column,concentrated by nitrogen blowing,filtered by 0.45 μm filter membrane,separated by Agilent ZORBAX SB-C_(18) column with the acetonitrile-0.2% formic acid aqueous solution(1:1,V:V) as mobile phase and isometric elution was performed at 0.3 mL/min,and quantified by external standard method.Results The selected ultraviolet detection wavelength was 254 nm,under this condition,the linear relationship between haloperidol concentration(X,μg/mL) and peak area(Y) was good in the range of 0.2-5.0 μg/mL,the correlation coefficient was 0.999,and the spiked recoveries at 3.0,7.0,10.0 μg/mL were 81.73%-95.57%,the relative standard deviation was 1.97%,the limit of detection was 7.58 μg/L,and limit of quantification was 25.27 μg/L.Conclusion This method has the advantages of low cost,simple operation,strong operability,high recovery,high sensitivity and high accuracy,which is suitable for the detection of haloperidol in milk.